CN1516204A - Method for making soft magnet silicon aluminium alloy powder core - Google Patents

Method for making soft magnet silicon aluminium alloy powder core Download PDF

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CN1516204A
CN1516204A CNA031148662A CN03114866A CN1516204A CN 1516204 A CN1516204 A CN 1516204A CN A031148662 A CNA031148662 A CN A031148662A CN 03114866 A CN03114866 A CN 03114866A CN 1516204 A CN1516204 A CN 1516204A
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alloy powder
bonding agent
quality
powder core
soft magnet
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CN1229826C (en
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刘善宜
祝家贵
柯昕
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Zhejiang east east Keda magnetoelectric Co., Ltd.
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HUZHOU KEDA MAGNETOELECTRICITY CO Ltd
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Abstract

The invention provides method to make a soft-magnetic inductance iron core by Fe-Si-Al alloy powder, including the steps: smelting Fe-Si-Al alloy - roughly crushing the cast ingot - heat treating - finely crushing into powder - annealing - grain mixing - passivating - adding insulating, binder, and mould-release agent - die forming - heat treating -coating surface. Its character: the binder is an epoxy one; the tempering after die forming is preserving the heat of the formed alloy powder at least 30 min on the condition of 600-800 deg.C nitrogen gas, argon gas or vacuum.

Description

The manufacture method of soft magnet silicon-aluminum powder core
[technical field]
The invention belongs to the manufacture method of magnetic bodies---particularly by the manufacture method of the soft magnetism inductor core of sendust stamping of powder moulding, this soft magnetism inductor core mainly is applicable to makes the iron core of stablizing inductor core, low noise filter and pulse transformer that transducer uses on the Switching Power Supply etc.
[background technology]
At present, along with the development of electron trade, various switch power converters, inverter, phase inverter etc. are widely applied magnetic permeability (μ in succession e) at the pure iron soft magnetic-powder core below 75, but there is the shortcoming that magnetic permeability is lower, temperature coefficient is bigger in the pure iron soft magnetic-powder core, is difficult to satisfy the requirement of technical development gradually; And the raw material costliness of the higher ferronickel magnetic core of magnetic permeability, technology are comparatively complicated, so valuable product, are difficult to penetration and promotion and use.
Soft magnet silicon-aluminum powder core is since 20th century, be found the thirties, with its higher resistivity with have higher magnetic permeability and extremely pay attention in low-intensity magnetic field.Therefore, it is designed to the occasion that the magnetic property requirement is higher than the pure iron soft magnetic-powder core; Again because its magnetic loss is lower, and energy storage capability is also higher than iron nickel molybdenum soft magnetic-powder core, become in the present Switching Power Supply store energy and filter inductor with the optimal selection material of magnetic core.
Existing method of producing soft magnet silicon-aluminum powder core comprises that---------fine crushing becomes alloy powder, and------grain size proportion---Passivation Treatment---adds insulating compound to annealing in process in alloy powder in heat treatment in the coarse crushing of sendust ingot casting for the smelting of sendust, bonding agent, release agent---compression molding---heat treatment---steps such as face coat, promptly smelting composition with Efco-Northrup furnace is silicon (Si) 8~12%, aluminium (Al) 4~7%, all the other are the alloy cast ingot of iron (Fe), broken and be heat-treated to alloy powder for twice through twice into stable mechanical performance, form according to certain particle afterwards and mix, carry out Passivation Treatment with potassium bichromate solution, surface at alloy powder forms coating film, in alloy powder, add insulating compound again, bonding agent, release agent, mixing and stirring, through granulation, pour mould compression moulding after the oven dry into, heat-treat at last, eliminate compacting stress, the surface that is coated in molded powder core with epoxy resin gets final product.Wherein used bonding agent is the sodium metasilicate inorganic adhesive, to carry out strict control to its use amount, too much can cause saturation flux density to reduce because use, used the mechanical strength that can cause the powder core at least to reduce, and in compression molding process after this, can increase the compacting drag, destroy the coating film on alloy powder surface, the performance of powder core is reduced; And organic class bonding agent usually produces cracking because of the high temperature that can not bear in the heat treatment process subsequently, so be excluded outside the scope of application.And the heat treatment process after the compression molding is normally carried out in the atmosphere of air or hydrogen, if in air, carry out, the easily oxidation of alloy powder surface; If select for use hydrogen as protective atmosphere, dangerous big, cost height, and easily make the embrittlement of powder core, cracky when coiling subsequently.
The flat 9-125108 of Japanese patent laid-open 9-74011 and Te Kai adopts the coreless induction furnace alloy smelting, in protective atmosphere, be atomized into powder, use, the insulation bonding of conventional sodium metasilicate, in the mist of nitrogen and hydrogen, carry out heat of reduction and handle the soft magnetic-powder core that can obtain better magnetic property alloy powder; Japanese patent laid-open 6-342714 uses silicone resin as bonding agent, 500~1100.Carry out the heat treatment after the compression molding in the C non-oxidizing atmosphere, the magnetic permeability that obtains soft magnetic-powder core only is 40; Japanese patent laid-open 11-189803 uses the poly-butyral resin of insulating properties bonding agent polyvinyl alcohol can obtain magnetic permeability (μ e) low-loss soft magnetic-powder core greater than 80.Above-mentioned several patents, though solved some particular problems the soft magnet silicon-aluminum powder core production technology from certain angle, its magnetic permeability is still less, and does not all relate to the drop performance of the alternating current-direct current stack of powder core.
[summary of the invention]
The technical assignment of the technical problem to be solved in the present invention and proposition is to overcome existing above-mentioned technological deficiency in the manufacture method of existing soft magnet silicon-aluminum powder core, the new slowly manufacture method that provides that a kind of technology powder core magnetic permeability comparatively convenient, that produce is higher, alternating current-direct current stack back magnetic property descends.
The present invention takes following technical proposals: a kind of manufacture method of soft magnet silicon-aluminum powder core, comprise the steps: the smelting of sendust---coarse crushing of sendust ingot casting---heat treatment---fine crushing becomes alloy powder---annealing in process---grain size proportion---Passivation Treatment---in alloy powder, add insulating compound, bonding agent, release agent---compression molding---heat treatment---face coat is characterized in that:
The bonding agent that is added after a, the Passivation Treatment is the epoxies bonding agent;
Temper after b, the compression molding is that molded alloy powder core is incubated 30 minutes at least in 600~800 ℃ nitrogen, argon gas or vacuum environment.
Compare with existing manufacture method, the present invention has following technique effect:
(1) bonding force is strong because bonding agent 607 epoxy resin, 609 epoxy resin, W-6A magnetic particle colloid stick and the W-6C magnetic particle colloid stick of epoxies has, the characteristics of good toughness, stable performance, can be dissolved in quickly in the solvent during concrete operations, drag during compacting and knockout press are than little with sodium metasilicate, promptly be easy to suppress, less to the wearing and tearing of mould, influence to magnetic property is less, contrast effect such as table 1 (data are the mean value of 50 samples):
Table 1
(2) select nitrogen, argon gas or vacuum protective gas for use as the compression molding after-baking, high safety, cost is low, is convenient to produce, and the not efflorescence of soft magnetic-powder core that produces, not cracking, mechanical strength height;
(3) soft magnetic-powder core that produces has the drop performance of good alternating current-direct current stack, i.e. after the alternating current-direct current stack, its magnetic property descends slowly.
Below the present invention is further illustrated.
[embodiment]
Embodiment one:
With Armco iron, silicon metal, fine aluminium drops into interior smelting of Efco-Northrup furnace of 50 kilograms of nominals, being cast into chemical composition is iron 84.80%, silicon 9.53%, the alloy cast ingot of aluminium 5.62%, with mechanical means the alloy cast ingot coarse crushing is become material piece below 25 millimeters, insert in the general reduction furnace with hydrogen shield atmosphere these material pieces and cooling after being incubated about 2 hours under the temperature conditions about 1200 ℃, further these material pieces are broken into material piece with jaw crusher again less than 6 millimeters, be ground into alloy powder below 100 orders with vibratory milling again, this alloy powder being inserted in the general reduction furnace with hydrogen shield atmosphere under the temperature conditions about 900 ℃ insulation carried out stress annealing in 1 hour and handles, screening afterwards, account for 20% according to 100~200 orders, 200~325 orders account for 28%, accounting for 52% mass ratio below 325 orders allocates the granularity of alloy powder, carry out Passivation Treatment with potassium bichromate solution afterwards, surface at alloy powder forms coating film, insulate with kaolin; Allocate the bonding agent glue afterwards, the absolute ethyl alcohol and the ethyl acetate that quality such as are about to mix, and slowly pour commercially available W-6A or W-6C magnetic bonding agent with quality such as absolute ethyl alcohol then in stirring into, to the three fully mutually dissolving promptly get glue; 2.4% the glue (0.8% W-6A or the W-6C magnetic bonding agent that promptly are equivalent to the alloy powder quality) that will be equivalent to the alloy powder quality is again poured in the alloy powder, fully mix, after the granulation oven dry, sieve less than 40 purpose powder, add zinc stearate again and make release agent, alloy powder is dropped in the mould of Φ 12.80/ Φ 7.20 * 5.0 (being that external diameter is that 12.80mm, internal diameter are that 7.20mm, thickness are the specification of the ring-type powder core of 5.0mm) with 1000~1200MPa (10~12T/cm 2) pressure compression moulding, the heat treatment of compacting stress was removed in insulation in 45 minutes in the vacuum about 1.5 handkerchiefs, 600 ± 15 ℃ the protective atmosphere heat-treatment furnace, painted the surface that is coated in the powder core with modified form epoxy resin at last and got final product.Its magnetic parameter such as table 2, table 3:
Table 2
Quality factor q 28.0 ????42.1 ????38.4 ????31.3 ????26.2
The inductance factors A L(nH/N 2) 58.5
Table 2 data show that the inductance factor of sample 1,2,3,4 is substantially at A L=56 * (1 ± 8%) nH/N 2Scope in, corresponding effective permeability (μ e) about 125, be higher than the performance of the soft magnetic-powder core of existing method manufacturing.
Table 3 (the DC stacked result of a-c cycle f=10KHz)
Figure A0311486600061
Table 3 data show that with the enhancing of stack direct current, the inductance value of sample 1,2,3,4 weakens slowlyer.
Embodiment two:
6.0% the glue (2.0% W-6A or the W-6C magnetic bonding agent that promptly are equivalent to the alloy powder quality) that will be equivalent to the alloy powder quality according to the processing step of embodiment one is poured in the alloy powder, all the other conditions are constant, get the soft magnetic-powder core of Φ 12.80/ Φ 7.20 * 5.0 specifications.Its magnetic parameter such as table 4, table 5:
Table 4
Figure A0311486600062
Quality factor q 28.0 ????40.3 ????31.3 ????26.2 ????21.9
The inductance factors A L(nH/N 2) 60.1
Table 4 data show that the inductance factor of sample 5,6,7,8 is substantially at A L=56 * (1 ± 8%) nH/N 2Scope in, corresponding effective permeability (μ e) about 125, be higher than the performance of the soft magnetic-powder core of existing method manufacturing.
Table 5 (the DC stacked result of a-c cycle f=10KHz)
Figure A0311486600071
Table 3 data show that with the enhancing of stack direct current, the inductance value of sample 5,6,7,8 weakens slowlyer.
Embodiment three:
9.0% the glue (3.0% W-6A or the W-6C magnetic bonding agent that promptly are equivalent to the alloy powder quality) that will be equivalent to the alloy powder quality according to the processing step of embodiment one is poured in the alloy powder, all the other conditions are constant, get the soft magnetic-powder core of Φ 12.80/ Φ 7.20 * 5.0 specifications.Its magnetic parameter such as table 6, table 7:
Table 6
Figure A0311486600072
Quality factor q 25.7 ????48.5 ????40.4 ????35.0 ????28.0
The inductance factors A L(nH/N 2) 53.9
Table 6 data show that the inductance factor of sample 9,10,11,12 is substantially at A L=56 * (1 ± 8%) nH/N 2Scope in, corresponding effective permeability (μ e) about 125, be higher than the performance of the soft magnetic-powder core of existing method manufacturing.
Table 7 (the DC stacked result of a-c cycle f=10KHz)
Table 7 data show that with the enhancing of stack direct current, the inductance value of sample 9,10,11,12 weakens slowlyer.
Embodiment four:
Processing step according to embodiment one, adjust the granularmetric composition of alloy powder, accounting for 12%, 200~325 orders according to 100~200 orders accounts for and accounts for 51% mass ratio below 37%, 325 orders granularity of alloy powder is allocated, all the other conditions are constant, the alloy powder compression molding is made the ring-type powder core that specification is Φ 20.87/ Φ 12.24 * 6.48, its magnetic parameter such as table 8, table 9:
Table 8
Figure A0311486600082
Table 8 data show that the inductance factor of sample 13,14 is substantially at A L=49 * (1 ± 8%) nH/N 2Scope in, corresponding effective permeability (μ e) about 90, be higher than the performance of the soft magnetic-powder core of existing method manufacturing.
Table 9 (the DC stacked result of a-c cycle f=10KHz):
Figure A0311486600091
Table 9 data show that with the enhancing of stack direct current, the inductance value of sample 13,14 weakens slowlyer.
Press the method step of embodiment one, two, three, four respectively, heat treatment temperature after the compression molding is changed between 600~800 ℃, as long as temperature retention time is no less than 30 minutes, the parameter of the magnetic parameter of gained soft magnetic-powder core and above-mentioned four embodiment contrasts respectively, change not quite fluctuation in the scope of above-mentioned parameter ± 8% basically; And change protective atmosphere simultaneously, use separately argon gas or nitrogen under normal pressure as protective gas, little to the influence of the magnetic property of soft magnetic-powder core.
Embodiment five:
According to the processing step of embodiment one,
During allotment bonding agent glue, the absolute ethyl alcohol and the ethyl acetate of quality such as use to mix, in stirring, slowly pour commercially available 607 or 609 epoxy resin with quality such as absolute ethyl alcohol then into, to the three dissolve fully mutually glue; All the other conditions remain unchanged, and mold pressing makes the ring-type powder core that specification is Φ 12.80/ Φ 7.20 * 5.0.Its magnetic parameter such as table 10, table 11:
Table 10
Figure A0311486600092
The inductance factors A L(nH/N 2) 59.3
Table 10 data show that the inductance factor of sample 15,16,17,18 is substantially at A L=56 * (1 ± 8%) nH/N 2Scope in, corresponding effective permeability (μ e) about 125, be higher than the performance of the soft magnetic-powder core of existing method manufacturing.
Table 11 (the DC stacked result of a-c cycle f=10KHz)
Table 11 data show, weaken slowlyer with the inductance value of the enhancing sample 15,16,17,18 of stack direct current.
Embodiment six:
6.0% the glue (2.0% 607 or 609 epoxy resin adhesives that promptly are equivalent to the alloy powder quality) that will be equivalent to the alloy powder quality according to the processing step of embodiment five is poured in the alloy powder, all the other conditions are constant, get the soft magnetic-powder core of Φ 12.80/ Φ 7.20 * 5.0 specifications.Its magnetic parameter such as table 12, table 13:
Table 12
Figure A0311486600102
Quality factor q 27.0 ????46.5 ????38.1 ????35.0 ????29.0
The inductance factors A L(nH/N 2) 57.2
Table 12 data show that the inductance factor of sample 19,20,21,22 is substantially at A L=56 * (1 ± 8%) nH/N 2Scope in, corresponding effective permeability (μ e) about 125, be higher than the performance of the soft magnetic-powder core of existing method manufacturing.
Table 13 (the DC stacked result of a-c cycle f=10KHz)
Table 13 data show that with the enhancing of stack direct current, the inductance value of sample 19,20,21,22 weakens slowlyer.
Embodiment seven:
9.0% the glue (3.0% 607 or 609 epoxy resin adhesives that promptly are equivalent to the alloy powder quality) that will be equivalent to the alloy powder quality according to the processing step of embodiment five is poured in the alloy powder, all the other conditions are constant, get the soft magnetic-powder core of Φ 12.80/ Φ 7.20 * 5.0 specifications.Its magnetic parameter such as table 14, table 15:
Table 14
Figure A0311486600112
Sample 26 Inductance value L (μ H) ????132.7 ????132.2 ????131.5 ????130.0 ????128.1
Quality factor q ????24.1 ????45.5 ????37.3 ????34.2 ????28.1
The inductance factors A L(nH/N 2) ????53.1
Table 14 data show that the inductance factor of sample 23,24,25,26 is substantially at A L=56 * (1 ± 8%) nH/N 2Scope in, corresponding effective permeability (μ e) about 125, be higher than the performance of the soft magnetic-powder core of existing method manufacturing.
Table 15 (the DC stacked result of a-c cycle f=10KHz)
Table 15 data show that with the enhancing of stack direct current, the inductance value of sample 23,24,25,26 weakens slowlyer.
Embodiment eight:
Processing step according to embodiment six, adjust the granularmetric composition of alloy powder, accounting for 12%, 200~325 orders according to 100~200 orders accounts for and accounts for 51% mass ratio below 37%, 325 orders granularity of alloy powder is allocated, all the other conditions are constant, the alloy powder compression molding is made the ring-type powder core that specification is Φ 20.87/ ф 12.24 * 6.48, its magnetic parameter such as table 16, table 17:
Table 16
Figure A0311486600122
Table 16 data show that the inductance factor of sample 27,28 is substantially at A L=49 * (1 ± 8%) nH/N 2Scope in, corresponding effective permeability (μ e) about 90, be higher than the performance of the soft magnetic-powder core made from existing method.
Table 17 (the DC stacked result of a-c cycle f=10KHz):
Table 17 data show that with the enhancing of stack direct current, the inductance value of sample 27,28 weakens slowlyer.
Press the method step of embodiment five, six, seven, eight respectively, heat treatment temperature after the compression molding is changed between 600~800 ℃, as long as temperature retention time is no less than 30 minutes, the parameter of the magnetic parameter of gained soft magnetic-powder core and above-mentioned four embodiment contrasts respectively, change not quite fluctuation in the scope of above-mentioned parameter ± 8% basically; And change protective atmosphere simultaneously, use separately argon gas or nitrogen under normal pressure as protective gas, little to the influence of the magnetic property of soft magnetic-powder core.
Need to prove, in the above-described embodiments:
For more more convenient, during allotment bonding agent glue, can in stirring, in acetone, slowly pour the epoxies bonding agent that quality is an acetone 1/2nd (commercially available W-6A magnetic bonding agent, W-6C magnetic bonding agent, 607 epoxy resin or 609 epoxy resin) into, to the two dissolve fully mutually glue; 2.4~9.0% the glue that will be equivalent to the alloy powder quality is again poured in the alloy powder, fully mixes, and the granulation oven dry, the final performance of products obtained therefrom does not have significant difference with using absolute ethyl alcohol and ethyl acetate.
Used protective atmosphere heat-treatment furnace can with tube furnace (horizontal), with box type furnace or vacuum furnace, not influence the final performance of product when (about 10Kg product) in enormous quantities during small lot (about 4Kg product) according to how much the selecting of treatment product.Wherein, vacuum furnace can directly use, and tube furnace and box type furnace can use at the two ends of inner bag increase air inlet/outlet (be used to vacuumize, or feed nitrogen or argon gas) by increasing stainless steel sealing inner bag.

Claims (5)

1, a kind of manufacture method of soft magnet silicon-aluminum powder core, comprise the steps: the smelting of sendust---coarse crushing of sendust ingot casting---heat treatment---fine crushing becomes alloy powder---annealing in process---grain size proportion---Passivation Treatment---in alloy powder, add insulating compound, bonding agent, release agent---compression molding---heat treatment---face coat is characterized in that:
The bonding agent that is added after a, the Passivation Treatment is the epoxies bonding agent;
Heat treatment after b, the compression molding is that molded alloy powder core is incubated 30 minutes at least in 600~800 ℃ nitrogen, argon gas or vacuum environment.
2, the manufacture method of soft magnet silicon-aluminum powder core according to claim 1 is characterized in that described epoxies bonding agent is 607 epoxy resin, 609 epoxy resin, W-6A magnetic particle colloid stick or W-6C magnetic particle colloid stick.
3, the manufacture method of soft magnet silicon-aluminum powder core according to claim 1 and 2, the quality that it is characterized in that adding after the Passivation Treatment epoxies bonding agent in alloy powder is 0.8~3.0% of an alloy powder quality.
4, the manufacture method of soft magnet silicon-aluminum powder core according to claim 3, when it is characterized in that in alloy powder, adding the epoxies bonding agent, absolute ethyl alcohol that quality is equated and ethyl acetate mix earlier, in stirring, slowly pour the epoxies bonding agent that equates with the absolute ethyl alcohol quality then into, to the three dissolve fully mutually glue; 2.4~9.0% the glue that will be equivalent to the alloy powder quality is again poured in the alloy powder, fully mixes the granulation oven dry.
5, the manufacture method of soft magnet silicon-aluminum powder core according to claim 3, when it is characterized in that in alloy powder, adding the epoxies bonding agent, in stirring, in acetone, slowly pour the epoxies bonding agent that quality is an acetone 1/2nd into, to the two dissolve fully mutually glue; 2.4~9.0% the glue that will be equivalent to the alloy powder quality is again poured in the alloy powder, fully mixes the granulation oven dry.
CN 03114866 2003-01-08 2003-01-08 Method for making soft magnet silicon aluminium alloy powder core Expired - Fee Related CN1229826C (en)

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